FERROXYL TEST FOR IRON CONTAMINATION

1. SCOPE

This specification describes a highly sensitive test for detecting free iron on surfaces
of equipment, and the preparation of the equipment for the test.

2. SAFETY PRECAUTIONS FOR DU PONT EMPLOYEES

MAKING INSPECTIONS IN SUPPLIERS' SHOPS

2.1 Acid-cleaning and ferroxyl solutions must be handled carefully and the following
precautions observed.

2.1.1 Safely goggles of the chemical type are to be worn when spraying, mixing, or
pouring acid or ferroxyl solution.

2.1.2 Solution must be kept form contact with the skin. Should contact occur
unavoidably, the skin must be washed immediately with water.

2.1.3 Hands are to be protected with rubber gloves.

2.1.4 If the solution is applied by spray gun in an enclosure, adequate protective

rubberized clothing shall be provided.

2.1.5 Employees should not breathe vapors of ferroxyl solution and adequate
protection always shall be provided when testing in a closely confined place.
This is to include masks supplied with air from an outside source that has been filtered
by an apparatus similar to the Purolator when such is available. If this filtering
equipment is not available, a self-contained air mask is required like the Scott Air Pak
or the Mine Safety Appliance Company's Chem-Ox. Fit testing of respirators is an
essential part of any protection program.

3. SAFETY PRECAUTIONS IN DU PONT PLANTS

3.1 When this specification is employed on Du Pont plants or construction sites, the
local safety rules shall govern in cases of conflict with this specification.

3.2 Both nitric and hydrofluoric acids emit highly toxic fumes when heated to
decomposition. The following is recommended.

3.2.1 Avoid welding when possible after ferroxyl testing.

3.2.2 In the event that welding becomes necessary after ferroxyl testing, all traces of
the ferroxyl solution must be completely removed.

3.2.3 Adequate ventilation must be provided. This is especially important when welding
in enclosed areas, such as vessels, etc.

4. GENERAL

4.1 Ferroxyl testing is effective for the following materials:

All AISI 200, 300, and 400 series
All Alloy 20 type material
Ni-Mo-Cr Alloy C-276 and C-4
Inconel and Incoloy
Precipitation hardening stainless steels
High-carbon, high-chromium(12% chromium) tool steels
Nichrome
Titanium
Chromium plating
Aluminum
4.2 Whenever this test is required, it shall be specified in the purchase order.
Fabricators of equipment shall indicate the items in the Bill of Material submitted to Du
Pont which are subject to such tests after fabrication.

4.3 Provisions are given for two levels of freedom from iron.

4.3.1 100 Percent Free. This shall be specified in the purchase order when equipment
must be absolutely devoid of all free iron. The test will be applied to 100 percent of the
surface which must be free from any indication of iron.

4.3.2 Less Than 100 Percent Free. This shall be specified in the purchase order when
a slight amount of iron contamination can be tolerated. The Du Pont engineer is to
consult with the Du Pont materials engineer to develop criteria for test.

4.4 The Du Pont inspector responsible shall witness the test.

5. SURFACE PREPARATION AND PROTECTION

5.1 Prior to ferroxyl tests, the equipment shall be thoroughly cleaned of foreign material.

5.2 The following procedures will help fabricators produce equipment which will meet
the requirements of this specification.

5.2.1 When closure of equipment is done by welding from one side only, as in the case
of butt or lap welds, the internal seams must be scal welded. Further, all internal
welded parts must be seal welded. Where fabrication conditions make seal welding
impossible, the fabricator must submit to Du Pont, in writing, a welding and cleaning
procedure for approval with quotation.

5.2.2 Weld surface must be as clean as the adjacent plate surfaces. All spatter and
slag must be removed, and cracks or porosity eliminated in advance of cleaning for
ferroxyl tests.

5.2.3 If wire brushes, steel wool, or similar agents are to be used in conditioning
surfaces, only such articles as were produced from Type 300 series stainless steel, and
are uncontaminated, shall be employed.

5.2.4 Grinding operations should be done only with aluminum oxide wheels that have
not been previously employed on carbon steels.

5.2.5 Wherever possible, stainless steel tools or accessories should be employed.

Carbon steel tools should be protected adequately from direct contact with the surfaces
to be later subjected to the ferroxyl test. This may be done with rubber, stainless steel,
or tape.

5.2.6 Forming rolls and dies should be inspected for undesirable projections that must
be dressed down before use. Contamination possibilities during forming operations
may be prevented, to a large extent, if paper or cardboard interlays are arranged
between the material and the rolls or dies. Shearing and forming brake tables should
be covered with paper to minimize the chance of contact between the carbon steel
surfaces and the fabricated material.

5.2.7 Clean rubber overshoes should be worn by workmen walking on equipment

surfaces or entering such equipment or tanks. Such overshoes should be used as little
as possible except for the purpose stated, and should be washed off frequently with a
pickling solution to preserve their cleanliness.

5.2.8 Dust that could contain free iron should be removed from the fabricated parts as
construction proceeds.

5.2.9 Castings should be molded in new sand restricted to this use, and neither
chaplets nor chill pins made of carbon steel are to be employed. Castings should be
steam cleaned and thoroughly rinsed with water after pickling.

5.2.10 All hydrostatic tests should be performed before preparing the surfaces for
ferroxyl testing.

5.2.11 A thorough detergent wash or steam cleaning followed by rinsing is normally

required on all surfaces prior to ferroxyl testing to assure freedom from iron
contamination.
5.3 If contamination is shown by test after such cleaning, use one of the following
methods for additional cleaning.

5.3.1 Degreasing. Greasy surfaces may contain free iron which remain after the
detergent wash. Degreasing is suggested to be followed by another detergent wash
and rinse.

5.3.2 If contamination appears to be the result of abrasive residues left by carbon steel
implements on the surfaces of the Type 300 or 400 series, or Alloy 20 Cb-3 materials,
the cleaning method employed to remove such contamination will depend upon the
composition and heat-treatment condition of the particular item.

5.3.2.1 Mill products or castings of any of the above compositions which are in the
solution-annealed condition or weldments of Types 304L, 316L, 321, 347, and No.20
Cb-3 may be cleaned by scrubbing with, or immersing in, a pickling solution composed
of:
10 percent by volume of 60-67 percent nitric acid;
1.3 percent by volume of 52 percent hydrofluoric acid; balance water
Under no conditions shall the pickling solution be allowed to contact the parts for more
than 30minutes at room temperature, or 15minutes at temperatures up to 150℉(66℃).

5.3.2.2 Weldments of Types 304, 316, or any of the other non-ELG, nonstabilized
grades or severely sensitized items(such as those which have been stress relieved) of
any of the grades(including ELC and stabilized) shall not be cleaned in HNO₃-HF
solutions. Suggested cleaning methods include blasting with previously unused, iron-
free sand or aluminum grit, and cleaning with milder acids such as 30 percent by
weight HNO₃at 150℉(66℃) max or 10 percent by weight oxalic at 150℉(66℃) max,
for a period not to exceed 15minutes.

5.3.2.3 The type 400 series stainless steels after pickling will contain a gray smudge.
This smudge must be removed by thorough washing using water, detergent, and scrub
brushes prior to ferroxyl testing. If this smudge in not completely removed, the ferroxyl
test will give a positive indication.
Note: The hardenable Type 400 series and the precipitation-hardened stainless steels
in the hardened condition are subject to hydrogen embrittlement. Whenever possible,
cleaning of these materials should be by mechanical methods. Plain nitric acid solution
or citric acid-sodium nitrate mixture is much less prone to cause hydrogen
embrittlement than nitric-hydrofluoric acid solution. If acid must be used, the parts
should be heated from 250 to 300℉(121 to 149℃) and held for 24hours after pickling.

5.3.3 Information concerning suitable pickling solution and procedures for the other
materials listed in 4.1 may be obtained from the suppliers of these materials.

5.3.4 If contamination is still present after pickling, sandblasting is suggested, using

sharp, clean, iron-free sand. Sand should not be reused and should come from
hoppers that were thoroughly cleaned before filling. Sandblasting of clad material
should not be carried to the point of seriously reducing the cladding thickness. Any
other blasting materials such as aluminum grit shall not have been used previously on
carbon steels.

6. TESTING AND INTERPRETATION OF RESULTS

6.1 Testing Solution

Distilled water 94% by wt 1000cc 1gal
Potassium 3% by wt 30g 4 ox
ferricyanide
Nitric acid (60-67℃) 3% by wt 20cc 1/5 pt

6.1.1 Because this solution will begin to discolor after mixing, it shall only be prepared
immediately prior to use.

6.2 Application of Solution and Interpretation of Results

6.2.1 Apply the solution with a spray atomizer made of plastic, rubber, glass, or
aluminum. Be certain that the atomizer contains no iron parts. The presence of iron will
be indicated by the solution turning to a dark blue color. If dark blue areas develop
within 30seconds after the solution has wetted the surface, the test is considered
positive and the contaminated areas must be cleaned and retested. Unless otherwise
stated, it is required that 100 percent of the area show a negative reaction in this test.
In either case, wash immediately to prevent blue stains from appearing on the surface.
Caution: Dark areas may appear after 30seconds and these results may be
misinterpreted.

6.2.1.1 Small parts may be tested by immersing in the solution. It the solution becomes
contaminated, it must be replaced. The solution must be washed from the parts
immediately after testing.

6.2.2 During ferroxyl testing, the solution is to be washed from the surfaces with water
as soon after the 30-second interval as possible. If water does not remove the stain on
the surface, a 10 to 20 percent solution of acetic acid or water-white vinegar can be
used, applied by a scrubbing action. CP ammonium hydroxide also may be used for
this purpose.

6.2.3 Waste Disposal Method. Disposal of in accordance with local, state, and federal
regulations.

6.2.4 Wipe surfaces dry with a clean white cloth after rinsing.

7. TUBULAR HEAT EXCHANGERS

7.1 When the ferroxyl test is to be applied, the order or drawings will specify whether
the tube side, shell side, or both, are to be tested. The test is to be made as with any
other equipment with the following exceptions.

7.1.1 Tube Side. The face of the tubesheet is to be tested in the usual manner. The
insides of the tubes are to be tested by inserting a swab saturated with the solution to a
distance extending approximately 1 inch beyond the roller area and then withdrawn. If
the characteristic
blue color appears on the swab, indicating iron contamination, the tube is to be
recleaned and retested until the test is negative.

7.1.2 Shell Side. The solution is to be sprayed on the outside of the tubes and
examination made as outlined in section 6. If, within 30seconds, any areas visible from
the outside of the bundle show iron contamination, those areas are to be recleaned and
retested until the test is negative.

7.1.3 Wipe surfaces dry with a clean white cloth after rinsing.

8. PREPARATION FOR SHIPMENT OR STORAGE

8.1 Immediately after the test, the equipment is to be dried and closed to avoid
contamination and damage during handling, shipping, and storage.

8.1.1 Small openings are to be sealed by completely covering with an adhesive tape
and this, in turn, protected by metal or waterproof plywood covers held in place with
bolts or steel banding.

8.1.2 Large openings, such as manholes, are to be covered with full iron-free gasket
disks and metal or waterproof plywood covers. The covers are to be completely sealed
with adhesive tape covering the flange and edges. Four or more bolts are to be
employed.

8.1.3 Large openings, such as the open ends of columns or open-top bins, are to be
closed by special methods. The proposed closure is to be briefly described in the
quotation. This is to be in the form of a sketch showing the arrangement and materials
to be used.

8.1.4 Small parts are to be packed in clean paper and boxes for protection.

8.2 Prior to shipment, the Du Pont inspector is to witness and approve the closure of all
ferroxyl tested equipment.

8.3 The closures or seals provided by the vendor are not to be disturbed or removed
until the adjoining equipment(pipe, agitator, instrument, etc) is to be physically
connected in the field. Care must be exercised to prevent the entry of any foreign
material, especially rust of other products of corrosion which may be in the vicinity.
9. SPECIAL MARKING

9.1 Any marking paint, inks, etc, used for purpose of identification shall not contain
harmful quantities of low-melting metals or metal salts such as zinc, lead, or cadmium
which can cause cracking during welding or heating, or of chlorides which can cause
stress-corrosion cracking.
Refer to SP3D or a materials engineer to ensure suitability of marking materials.

9.2 In addition to the marking required by other applicable specifications,

equipment(such as tanks) which has been tested and can be closed shall have the
statement "FERROXYL TESTED - DO NOT REMOVE SEALS" painted on the outside
in a conspicuous place in letters at least 6 inches high, where practical. Parts which are
crated or boxed shall have the crate or box similarly marked. Other parts which are
shipped loose shall be tagged, the tag being marked as above.